CN100429180C - 堇青石材质蜂窝结构体的制造方法 - Google Patents
堇青石材质蜂窝结构体的制造方法 Download PDFInfo
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Abstract
提供能够抑制烧成时的裂纹产生的堇青石材质蜂窝结构体的制造方法。该堇青石材质蜂窝结构体的制造方法具有:制作含有长宽比大于或等于1.5的堇青石化原料的坯土的工序、将上述坯土成型制作蜂窝形状的成型体的工序、干燥上述成型体制作蜂窝干燥体的工序、以及将上述蜂窝干燥体烧成制作堇青石材质蜂窝结构体的工序。
Description
技术领域
本发明涉及堇青石材质蜂窝结构体的制造方法,更详细地说,是关于能够提高蜂窝干燥体的强度、抑制烧成时的裂纹产生的蜂窝结构体的制造方法。
背景技术
考虑到对环境的影响,从排气中除去内燃机、锅炉等排出的气体中的微粒或有害物质的必要性提高。尤其是关于除去从柴油发动机排出的微粒(以下往往称为“PM”)的规制,在世界范围内有强化的倾向,作为用于除去PM的捕集过滤器(柴油机微粒过滤器,以下往往称为“DPF”),由蜂窝结构体构成的过滤器(蜂窝过滤器)的使用受到注目,提出了种种体系。上述DPF的构造通常如下:由多孔分隔壁划分形成多个作为流体流路的孔道,通过将孔道交替地封堵,构成孔道的多孔分隔壁起到过滤器的作用。另外,作为DPF的材质,适合使用热膨胀系数小、耐热冲击性高的堇青石。
由这样的蜂窝结构体构成的蜂窝过滤器,虽然被安装在柴油发动机的排气系统中使用,但由于柴油发动机搭载在卡车或公共汽车等大型车辆上,因而排气量大,也就需要蜂窝结构体大型化、薄壁化。但是,当蜂窝结构体大型化、薄壁化时,在其制造过程中,存在烧成时分隔壁产生裂纹这样的问题。
另一方面,在不是堇青石材质,而是碳化硅材质的蜂窝过滤器的制造中,公开了使一部分原料粉末的圆形度达到小于或等于0.85,在抑制制造时的翘曲,维持弯曲强度的同时,提高气孔率的制造方法(例如参照特开2002-293660号公报)。但是,作为制造大型化和/或薄型化的堇青石质蜂窝结构体的方法,即使使其原料的圆形度达到小于或等于0.85,也未必能够抑制制造时的裂纹。
发明内容
本发明就是鉴于现有技术存在的这样的问题而完成的,其特征在于,提供能够提高蜂窝干燥体的强度、抑制烧成时的裂纹产生的堇青石材质蜂窝结构体的制造方法为特征。
按照本发明,提供以下的堇青石材质蜂窝结构体的制造方法。
(1)堇青石材质蜂窝结构体的制造方法,该方法具有制作含有长宽比1.5~5的堇青石化原料的坯土的工序、将上述坯土成型制成蜂窝形状的成型体的工序、干燥上述成型体制作蜂窝干燥体的工序、以及将上述蜂窝干燥体进行烧成制作堇青石材质蜂窝结构体的工序。其中,相对于上述坯土所含的堇青石化原料全体,长宽比为1.5~5的堇青石化原料的含量为5~40质量%;且长宽比为1.5~5的堇青石化原料是平均短径为0.5~5μm的纤维状氧化铝、平均短径为1~20μm的纤维状硅铝酸盐或者平均短径为1~20μm的纤维状二氧化硅;且堇青石化原料的平均粒径为0.5~100μm。
(2)如(1)中记载的堇青石材质蜂窝结构体的制造方法,其中,上述长宽比大于或等于1.5的堇青石化原料是纤维。
(3)如(1)或(2)中记载的堇青石材质蜂窝结构体的制造方法,其中,上述长宽比大于或等于1.5的堇青石化原料是氧化铝、硅铝酸盐或者二氧化硅。
(4)如(1)~(3)任一项中记载的堇青石材质蜂窝结构体的制造方法,其中,相对于上述坯土中含有的全部堇青石化原料,上述长宽比大于或等于1.5的堇青石化原料的含量为大于或等于5质量%。
(5)如(1)~(4)任一项中记载的堇青石材质蜂窝结构体的制造方法,其中,上述坯土含有长宽比大于或等于2的堇青石化原料。
(6)如(1)~(4)任一项中记载的堇青石材质蜂窝结构体的制造方法,其中,上述坯土含有长宽比大于或等于3的堇青石化原料。
(7)由(1)~(6)任一项中记载的堇青石材质蜂窝结构体的制造方法得到的堇青石材质蜂窝结构体。
发明效果
按照本发明的堇青石材质蜂窝结构体的制造方法,由于使用含有长宽比大于或等于1.5的堇青石化原料的坯土制作蜂窝成型体,并将其干燥为蜂窝干燥体,因而,原料相互间的接触面积变大、原料相互的缠绕变得更强,因此蜂窝干燥体的强度得到提高。而且在烧成蜂窝干燥体来制作堇青石材质蜂窝结构体时,烧成所引起的裂纹的产生被抑制。
具体实施方式
以下,具体地说明用于实施本发明的最佳方式(以下,称为“实施方式”),但本发明不受以下的实施方式的限制,应该理解为,在不脱离本发明的宗旨的范围,基于本领域技术人员的常识,还可进行适宜设计的变更、改进等。
本发明的堇青石材质蜂窝结构体制造方法的一种实施方式是具有:制作含有长宽比大于或等于1.5的堇青石化原料的坯土的工序、将上述坯土成型制作蜂窝成型体的工序、干燥上述成型体制作蜂窝干燥体的工序、以及将上述蜂窝干燥体烧成制作堇青石材质蜂窝结构体的工序。这里,所谓长宽比是原料粒子的长径除以原料粒子的短径的所得的值,以下式表示。
长宽比=(原料粒子的长径)/(原料粒子的短径)
而长宽比的测定,通过对堇青石化原料进行SEM(扫描电子显微镜)照相得到的的图像进行图像解析来进行。这里,所谓原料粒子的短径,是指经过能够以SEM照相辨别的原料粒子的重心的最短的长度(径),所谓长径,是指经过能够以SEM照相辨别的原料粒子的重心的最长的长度(径)。
上述坯土含有长宽比大于或等于1.5的堇青石化原料,但并不是所有堇青石化原料的长宽比都必须大于或等于1.5。也就是说,只要至少一部分堇青石化原料的长宽比大于或等于1.5就可以。进而,优选至少一部分堇青石化原料的长宽比大于或等于2,更优选大于或等于3,尤其优选大于或等于3.5。由于含有长宽比大于或等于1.5的堇青石化原料,在制作蜂窝干燥体时,原料相互间的接触面积就变大,原料相互间的缠绕变得更强,因此蜂窝干燥体的强度提高。因而,在烧成蜂窝干燥体制作堇青石材质蜂窝结构体时,能够达到抑制烧成引起的裂纹的产生。因而,能够提高堇青石材质蜂窝结构体制造的合格率,提高生产速度,削减制造成本。另外,上述长宽比大于或等于1.5的堇青石化原料的长宽比的上限虽然没有特别的限制,但最好是小于或等于5.0。当超过5.0时,坯土的流动性受损,在挤出成型时有带来故障的担心。
上述长宽比大于或等于1.5的堇青石化原料,优选是纤维。原因在于,在制作堇青石材质蜂窝结构体的工序中,较之使用长宽比大于或等于1.5的棒状的粒子等,能够更提高蜂窝干燥体的强度。这里,所谓纤维,是将原料加热至熔点以上,拉伸成纤维状所得到的针状粒子形状的原料。
上述长宽比大于或等于1.5的堇青石化原料,相对于堇青石化原料全体,其含量优选为大于或等于5质量%,更优选为7~40质量%,尤其优选为15~30质量%。如果少于5质量%,则往往难以提高蜂窝干燥体的强度。此外,如果大于40质量%,则有坯土流动性受损,给挤出成型造成障碍的担心。
在本实施方式中,作为堇青石化原料,可以从滑石、氧化铝、硅铝酸盐、氢氧化铝、二氧化硅、高岭土、莫来石、尖晶石等中选择,通过烧成而成为堇青石的组成加以使用。这些之中,优选含有长宽比大于或等于1.5的氧化铝、长宽比大于或等于1.5的硅铝酸盐或者长宽比大于或等于1.5的二氧化硅。进而为了更提高蜂窝干燥体的强度,对于长宽比大于或等于1.5的堇青石化原料,优选原料粒子的平均短径(以下仅称为“短径”)是0.5~5μm的纤维状氧化铝、平均短径是1~20μm的纤维状硅铝酸盐或者平均短径是1~20μm的纤维状二氧化硅。上述纤维状氧化铝等的平均短径如果比各自的下限值短,在挤出成型时就有发生故障的担心,如果比各自的上限值长,就有得不到目的的低热膨胀系数的担心。堇青石化原料的平均粒径优选是0.5~100μm,最优选是1~50μm。如果小于0.5μm,在挤出成型时就有发生故障的担心,如果大于100μm,就有得不到目的的低热膨胀系数的担心。
在本实施方式的堇青石材质蜂窝结构体的制造方法中,除了上述的堇青石化原料以外,还可以混合粘合剂、造孔剂、表面活性剂、增塑剂等来制作坯土。
在本实施方式中,从上述原料选择规定的原料进行混合,加水进行混炼而得到坯土。混合原料的方法,没有特别的限制,可以使用通常使用的搅拌器等。另外,混炼方法也没有特别的限制,可以使用通常使用的捏合机等。优选水是总坯土的15~35质量%。
接着,将由上述坯土制造方法得到的坯土成型,制作蜂窝形状的成型体。使坯土成型的方法没有特别的限制,可以通过挤出成型等进行。所得到的坯土,在使用挤出成型机进行成型之前,可以使用真空和泥机成型为圆柱状。
随后,干燥所得到的蜂窝形状的成型体,来制作蜂窝干燥体。作为干燥的方法,没有特别的限制,优选热风干燥、微波干燥等。热风干燥和微波干燥也可以同时进行,也可在进行一种干燥后,进行另一种干燥,或者也可只进行一种干燥。作为干燥条件,没有特别的限制,例如在50~150℃加热10~100分钟。
接着,根据需要将得到的蜂窝干燥体切断成规定的尺寸。然后,在作为DPF等的壁流式蜂窝过滤器时,可以将孔道交替地封堵。作为形成封堵的方法,例如在蜂窝干燥体的两端面贴附掩蔽膜,在相当于规定的孔道的位置开孔,在开孔的部分(孔道)注入封堵材料而形成封堵。作为封堵材料,优选使用和作为堇青石材质蜂窝结构体的原料的堇青石化原料相同的堇青石化原料。
如上所述,根据需要,将得到的蜂窝干燥体切断,形成封堵后,在规定的条件下进行烧成,就能够得到多孔的堇青石材质蜂窝结构体。作为烧成条件,没有特别的限制,例如在1350~1450℃加热1~10小时。
在蜂窝成型体(或者干燥体)的烧成中,在某一温度范围(150~800℃),处于粘合剂等发生燃烧、粘合剂等被除去的状态,而且处于还未成为堇青石材质的状态(堇青石化原料的状态)。此时,由于不存在粘合剂,因此处于蜂窝形状(分隔壁)容易崩溃的状态。在本实施方式中的堇青石材质蜂窝结构体的制造方法中,堇青石化原料中的至少一部分是长宽比大于或等于1.5,原料相互间的结合力强,因此即使是像这样易崩溃的蜂窝结构体,也能够维持其形状。而且,在其烧成过程中,能够抑制裂纹产生。
由本实施方式的堇青石材质蜂窝结构体的制造方法得到的堇青石材质蜂窝结构体的构造没有特别的限制。例如能够得到气孔率15~80%、平均气孔径1~40μm、孔道密度10~300孔/cm2、分隔壁厚度30~1000μm的堇青石材质蜂窝结构体。
另外,采用本实施方式的堇青石材质蜂窝结构体的制造方法,能够一面抑制裂纹产生等、一面制造体积大于或等于2000cm3的堇青石材质蜂窝结构体,进而能够一面抑制裂纹产生等、一面制造体积大于或等于2470cm3的堇青石材质蜂窝结构体。由本实施方式的堇青石材质蜂窝结构体的制造方法得到的堇青石材质蜂窝结构体的大小的上限没有特别的限制,但优选小于或等于40000cm3。这里,所谓堇青石材质蜂窝结构体的体积是指包括孔道和细孔的空间的堇青石材质蜂窝结构体整体的体积。
本发明的一种实施方式的堇青石材质蜂窝结构体的,是由上述本发明的堇青石材质蜂窝结构体的制造方法得到的堇青石材质蜂窝结构体。而且本实施方式的堇青石材质蜂窝结构体,能够适合作为蜂窝过滤器使用。以本实施方式的堇青石材质蜂窝结构体作为蜂窝过滤器使用,就能够得到由如上所述的体积大于或等于2000cm3、更优选是大于或等于2470cm3的堇青石材质蜂窝结构体构成的蜂窝过滤器。像这样,作为蜂窝过滤器使用由上述本发明的堇青石质蜂窝结构体的制造方法得到的体积大于或等于2000cm3、更优选是大于或等于2470cm3的堇青石材质蜂窝结构体,就能够一面抑制裂纹产生等、一面高效地制造用于卡车或公共汽车等的大型柴油发动机的蜂窝过滤器。
以下,根据实施例更具体的说明本发明,但本发明不限于这些实施例。
实施例1~4、实施例8、对比例1~3
作为堇青石化原料,使用19质量%的平均粒径10μm的高岭土、40质量%的平均粒径30μm的滑石、13质量%的平均粒径30μm的熔融二氧化硅、8质量%的平均粒径3μm的氢氧化铝、20质量%的表1记载的各个氧化铝(实施例1~4、实施例8、对比例1~3)的组合物。在组合物中加入6质量%的粘合剂(以得到的坯土全体作为100质量%时的比率),用螺旋桨式分配混合器混合3分钟,作为造孔材料添加使用20质量%(以得到的坯土全体作为100质量%时的比率)的平均粒径40μm的碳,再用螺旋桨式分配混合器混合3分钟。然后,在得到的混合物中喷雾添加24质量%(以得到的坯土全体作为100质量%时的比率)的水,再用螺旋桨式分配混合器混合3分钟后,用SIGMA捏合机混炼30分钟,得到坯土。
接着用真空和泥机将得到的坯土成型成圆柱状坯土,用活塞式挤出成型机成型成蜂窝形状。得到的蜂窝形状的成型体进行微波干燥,再进行热风干燥就得到蜂窝干燥体。得到的蜂窝干燥体切断成规定的尺寸,使用将堇青石化原料浆化而得到的封堵材料,以锯齿形格子状交替地进行封堵,在氧化气氛下于1420℃烧成6小时,得到堇青石材质蜂窝结构体(孔道构造:肋厚(分隔壁厚)0.3mm、孔道数47孔/cm3,尺寸:Φ144mm×长152mm)。
实施例5~7
作为堇青石化原料之一的氧化铝,组合使用实施例1中使用的纤维状氧化铝和对比例2中使用的粒状氧化铝,除此之外,和实施例1同样地制作,制成堇青石材质蜂窝结构体。氧化铝的组成如表1中所记载。
实施例9
作为堇青石化原料,除使用17质量%的平均粒径10μm的高岭土、43质量%的平均粒径30μm的滑石、13质量%的表2中记载的平均粒径24μm的纤维状二氧化硅以及27质量%的表2中记载的平均粒径6μm的纤维状氧化铝的组合物外,其余和实施例1一样地制作堇青石材质蜂窝结构体。
测定实施例1~7、对比例1~3所示的堇青石材质蜂窝结构体的制造工序中得到的蜂窝干燥体的原料强度(KPa)。作为测定方法,将蜂窝干燥体加工成直径25mm、高25mm,在700℃煅烧,然后测定结构体的流体流路方向的压缩强度。测定中使用的装置是岛津制作所生产的auto graph AG-25TA。测定结果示于表1及表2。
对各原料进行SEM照相,通过图像解析,测定长宽比。另外,各原料的平均粒径,使用堀场制作所生产的粒度分布测定机LA-910进行测定。测定结果示于表1及表2。
所得到的堇青石质蜂窝结构体的气孔率,使用玛库罗美利泰库斯(マイクロメリテイツクス)公司生产的水银压入式孔率计AutoPoreIII测定细孔总容积(cm3/g),按照下式计算:
气孔率=细孔总容积/(细孔总容积+1/2.52)×100
以堇青石的真比重作为2.52g/cm3。另外,平均细孔径,使用玛库罗美利泰库斯公司生产的水银压入式孔率计AutoPoreIII测定。测定结果示于表1及表2。
采用实施例1~7、对比例1~3的堇青石材质蜂窝结构体的制造方法,分别制作各10个堇青石材质蜂窝结构体,确认裂纹的产生情况。即使有一点细裂纹,也作为产生裂纹。结果示于表1及表2。
从表1可知,如果比较实施例1~7和对比例1~3,作为堇青石化原料的一部分含有长宽比大于或等于1.5的纤维状氧化铝的实施例1~7,蜂窝干燥体的原料强度都高于对比例1~3,烧成裂纹产生个数也少。另外,如果比较实施例1~4,就可知纤维状氧化铝的长宽比越高,蜂窝干燥体的原料强度越高。再比较实施例1、5~7,就可知长宽比3.5的纤维状氧化铝的含有率越高,蜂窝干燥体的原料强度越高。而且,还知道,长宽比3.5的纤维状氧化铝的含有率如果小于5,烧成裂纹产生个数,作为个数虽然少,但处于增加的倾向。
产业上的应用可能性
按照本发明的堇青石材质蜂窝结构体的制造方法,即使使蜂窝结构体大型化、薄壁化,在其制造过程中,也能够抑制烧成时的分隔壁的裂纹产生。由此在堇青石材质蜂窝结构体的制造中,能够提高其合格率、生产速度,削减制造成本。
Claims (3)
1.堇青石材质蜂窝结构体的制造方法,其具有:制作含有长宽比为1.5~5的堇青石化原料的坯土的工序、将上述坯土成型制作蜂窝形状的成型体的工序、干燥上述成型体制作蜂窝干燥体的工序、以及将上述蜂窝干燥体烧成制作堇青石材质蜂窝结构体的工序;
其中,相对于上述坯土所含的堇青石化原料全体,长宽比为1.5~5的堇青石化原料的含量为5~40质量%;且
长宽比为1.5~5的堇青石化原料是平均短径为0.5~5μm的纤维状氧化铝、平均短径为1~20μm的纤维状硅铝酸盐或者平均短径为1~20μm的纤维状二氧化硅;且
堇青石化原料的平均粒径为0.5~100μm。
2.根据权利要求1所述的堇青石材质蜂窝结构体的制造方法,其中,上述坯土含有长宽比为2~5的堇青石化原料。
3.根据权利要求1所述的堇青石材质蜂窝结构体的制造方法,其中,上述坯土含有长宽比为3~5的堇青石化原料。
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US7445745B2 (en) * | 2004-08-03 | 2008-11-04 | Corning Incorporated | Method for fabricating ceramic articles |
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2004
- 2004-03-23 JP JP2004083861A patent/JP4358662B2/ja not_active Expired - Fee Related
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2005
- 2005-03-18 US US11/082,979 patent/US7364689B2/en active Active
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Patent Citations (5)
Publication number | Priority date | Publication date | Assignee | Title |
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EP0554104A2 (en) * | 1992-01-30 | 1993-08-04 | Ngk Insulators, Ltd. | Ceramic honeycomb structure with grooves and outer coating and process of producing the same |
JPH07149579A (ja) * | 1993-11-26 | 1995-06-13 | Matsushita Electric Ind Co Ltd | コージェライト質多孔性セラミックス又はそれを用いたディーゼルエンジン用排ガスフィルターの製造方法 |
JPH07206540A (ja) * | 1994-01-19 | 1995-08-08 | Matsushita Electric Ind Co Ltd | コージェライト質多孔質耐熱材の製造方法 |
JPH09263465A (ja) * | 1996-03-29 | 1997-10-07 | Nagano Pref Gov | 軽量耐火物およびその製造方法 |
US20030110744A1 (en) * | 2001-12-13 | 2003-06-19 | Gadkaree Kishor P. | Composite cordierite filters |
Also Published As
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JP2005272158A (ja) | 2005-10-06 |
US7364689B2 (en) | 2008-04-29 |
JP4358662B2 (ja) | 2009-11-04 |
CN1680216A (zh) | 2005-10-12 |
US20050212186A1 (en) | 2005-09-29 |
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